A method for preparing 1-fluoronaphthalene by electrochemical fluorination

A fluorination method and electrochemical technology, applied in the field of electrochemistry, can solve the problems of increasing the concentration of nitrous acid, difficult operation, poor temperature control, etc., and achieve simple and easy production process, low equipment requirements, and high safety factor Effect

Inactive Publication Date: 2021-07-30
石家庄保利农化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sodium nitrite used in the diazotization reaction is a secondary inorganic oxidant, which decomposes at 175°C and can cause combustion or explosion of organic matter; It will increase the concentration of nitrous acid, accelerate the decomposition of materials, produce a large amount of oxygen gas, and cause the danger of explosion and fire
Poor temperature control, prone to accidents, difficult to operate, low safety factor
[0005] 2. The amount of waste water is large and the cost is high
Because a large amount of sulfuric acid is used in the reaction process, a large amount of strong acid wastewater will be generated, and the temporary storage of strong acid wastewater has potential safety hazards, and the treatment of a large amount of strong acid wastewater will also increase the cost, resulting in high cost
[0006] 3. The process is cumbersome, and the product must be obtained through three or four steps of reaction

Method used

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  • A method for preparing 1-fluoronaphthalene by electrochemical fluorination
  • A method for preparing 1-fluoronaphthalene by electrochemical fluorination
  • A method for preparing 1-fluoronaphthalene by electrochemical fluorination

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Experimental program
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Effect test

Embodiment 1

[0031] Materials: naphthalene 100g, acetonitrile 900g, tetramethylammonium fluoride hydrofluoride 2000g

[0032] Operation: Pour anhydrous acetonitrile into the electrolytic cell, the room temperature is 16 degrees Celsius, add naphthalene under stirring at 1000 rpm, after dissolving, add tetramethylammonium fluoride hydrofluoride, connect the power supply, platinum as the anode material, carbon Make cathode material, power on (constant voltage 2V, current 2-10mA), 10 hours of sampling and control, no product.

Embodiment 2

[0034] Materials: naphthalene 100g, acetonitrile 900g, pyridine hydrofluoride 2000g

[0035] Operation: Pour anhydrous acetonitrile into the electrolytic cell, the room temperature is 16 degrees Celsius, add naphthalene under stirring at 1000 rpm, after dissolving, add pyridine hydrofluoride, connect the power supply, use platinum as the anode material, and carbon as the cathode material, and power on (Constant voltage 2V, current 2-10mA), 10-hour sampling control, no product.

Embodiment 3

[0037] Materials: 900g acetonitrile, 100g naphthalene, 2000g triethylamine trihydrofluoride

[0038] Operation: Pour anhydrous acetonitrile into the electrolytic cell, the room temperature is 16 degrees Celsius, add naphthalene under stirring at 1000 rpm, after dissolving, add triethylamine trihydrofluoride, connect the power supply, use platinum as the anode material, and carbon as the cathode Materials, electricity (constant voltage 2V, current 2-10mA), after 10 hours of reaction, the yield of 1-fluoronaphthalene reached 25%. (See Figure 1-7 ).

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Abstract

The invention relates to a method for preparing 1-fluoronaphthalene by electrochemical fluorination, which comprises the following steps: adding a solvent into an electrolytic cell, turning on the stirring, adding substrate naphthalene, adding a fluorine source after completely dissolving, and connecting electrode sheets, Turn on the power supply, stir and react at a constant temperature to obtain 1-fluoronaphthalene. The invention has simple equipment, low equipment requirements, mild fluorination reaction conditions, no highly toxic or dangerous reagents, and can reduce pollution.

Description

technical field [0001] The invention relates to the field of electrochemical technology, in particular to a method for preparing 1-fluoronaphthalene by electrochemical fluorination. Background technique [0002] 1-Fluoronaphthalene is a drug intermediate developed in recent years. Since fluorine is the most active non-metallic element with the strongest electronegativity and its radius is similar to that of hydrogen atoms, when fluorine atoms are introduced into the drug, it has a A series of special properties, such as mimicry effect, lipophilicity, stability and so on. Therefore, many fluorine-containing drugs have lower toxicity, higher drug efficacy, stronger metabolism, and longer-lasting drug properties than fluorine-free drugs. Therefore, at present, fluorine-containing fine chemicals appear in various aspects of national defense and industrial production, and a group of fluorine-containing compounds with physiological activity have been successfully applied in the f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/11C25B3/28
CPCC25B3/28
Inventor 赵闯
Owner 石家庄保利农化工有限公司
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